Developed model for reduction mechanism of

iron ore pellets under load

K. S. Abdel-Halim*, M. I. Nasr and A. A. El-Geassy
A laboratory scale shaft furnace for testing the reduction of commercial iron ore pellets under load
was constructed. A series of reduction experiments of iron ore pellets with a synthetic reformed
natural gas was carried out under various operational conditions of varying temperature, type of
ore pellets and applied load. The reduction tests were carried out at 750–1000uC under different
loads, i.e. 0?2, 0?4 and 0?57 kg cm22. The sticking phenomenon accompanying reduction of iron
ore pellets under load was investigated and was found to be dependent on temperature,
chemical composition and applied load. The experimental results were analysed to investigate
the reduction kinetics and mechanism of iron ore pellets under controlled conditions of
temperature and applied load. A model was developed depending on the shrinking core modulus
and mixed control ratio to give a definite and quantified measure of reduction reaction. This model
allows good analysis of the actual effect of reduction temperature and applied load upon
controlling mechanism and furthermore, it indicates the relative effect of the different mechanisms
in the mixed control regime.
Keywords: Iron ore pellets, Shaft furnace, Direct reduction, Kinetics and mechanism, Sticking, Reduction under load

Introduction comparative study on the effect of reduction tempera-

Reduction processes of iron oxides include many
complicated reactions and take place in a stepwise
manner via formation of a series of intermediate oxides.
The reduction behaviour of iron oxides using gases or
solid reductant has been extensively studied under
isothermal and non-isothermal conditions.1–5 In a real
shaft furnace, the reduction processes of iron ore pellets
or lumps are usually undertaken under load where the
upper charge layers are exerting load upon the lower
layers. A few attempts have been made to simulate the
reduction operation in shaft furnaces under load.6–9 The
reduction under load test was discussed in the literature7
and the results obtained were used for determining the
quality control of the pellets produced for direct
reduction processes. Khaki et al.8 used six types of self
fluxed pellets in reduction experiments under load. The
reducibility of each pellet was affected by its original
characteristics and increased with increasing porosity
and decreasing slag-forming amount.
On the other hand, the reduced pellets were stuck
together forming clusters during reduction process
under load. The sticking of pellets during reduction is
mainly dependent on temperature, time, chemical
constituents and the load applied. Ekpe and Walker10
determined the clustering tendencies of compacts using a
tensometer modified for reduction under load tests. A
Central Metallurgical Research & Development Institute (CMRDI), PO Box
87, Helwan, Cairo, Egypt
*Corresponding author, email khsaad99@yahoo.com
ture and time on the structure of hematite and magnetite
was made by Nasr.11 He observed that as the induration
time increased, more bridging happened between parti-
cles, forming a cluster nucleus which became much more
developed with sintering and grain growth of particles.
Kodak et al.12 investigated the mechanism of the
agglomeration of iron ore pellets under load using
hydrogen gas. They found that the contact strength
increased with temperature, extent of reduction and
external load. The effect of compacting pressure,
sintering temperature and time on density and structural
characteristics of the sintered iron compacts has been
investigated by Omar et al.13 Compact density increased
with the increase in compacting pressure and sintering
time. Although sintering temperature increases the
densification for both a- and c-Fe phases, the effect is
much more pronounced in the a-Fe than in c-Fe phases.
The changes in pore structure which occur during
sintering process are of fundamental importance to the
reduction kinetics and mechanical properties of agglom-
erates.14,15 The different factors affecting high tempera-
ture properties of iron ore compacts such as porosity,
temperature, slag former amounts and basicity were also
investigated.16–19
In related investigations for the authors, the isother-
mal reduction behaviour of iron ore pellets under load
was investigated at 1023–1273 K.20,21 Experimental runs
were performed to investigate the reduction kinetics and
mechanism under controlled conditions of temperature
and applied load. It was found that the load had a
measurable effect on the reduction due to the sintering

ß 2011 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 16 June 2009; accepted 6 June 2010
DOI 10.1179/030192310X12816231892305 Ironmaking and Steelmaking 2011 VOL 38 NO 3 189
Abdel-Halim et al. Developed model for reduction mechanism of iron ore pellets

Table 1 Physicochemical characteristics of fired fluxed iron ore pellets

Chemical composition, mass-% Physical characteristics

Acidic Basic Acidic Basic

Fe2O3 96.57 96.23 Average porosity, vol.-% 32 34

SiO2 1.46 0.95 Average diameter, mm 12.85 13.1
CaO 0.59 1.15 Pore area, m2 g21 0.517 0.612
MgO 0.30 0.80 Bulk density, g cm23 3.43 3.67
Al2O3 0.93 0.25
FeO 0.09 0.25
S 0.002 0.01
P 0.091 0.03
TiO2 0.020 0.30

of freshly formed metallic iron that increased with
temperature and reduction extent.
The present study is designed to investigate the
influence of the reduction parameters of temperature,
load applied and chemical composition on the structural
changes accompanying sticking of high grade iron ore
pellets. A developed model was demonstrated to study
the effect of reduction conditions on the kinetics and
mechanism of reduction of iron oxide pellets under load.
Experimental
The physical and chemical characteristics of two types of
fluxed iron ore pellets are given in Table 1. The basicity
of pellets in terms of (CaOzMgO) and (SiO2zAl2O3) is
0?37 and 1?62 indicating that the former is acidic while
the later is basic. These pellets were isothermally reduced
at 750–1000uC in synthetic gas mixture composed of
55%H2, 36%CO, 5%H2O, 3%CO2 and 1%N2. This gas
mixture represents the actual composition of reformed
natural gas used in Midrex processes at ANSDK
(Alexandria, Egypt). The reduction experiments were
carried out under different loads ranging from 0 to
0?57 kg cm22. The course of reduction was followed by
measuring the weight loss as a function of time under
controlled operational conditions. The schematic dia-
gram for the system used for carrying out the reduction
experiments is given elsewhere.20 In order to have
detailed information about the microstructure of the
pellets reduced under load, an optical microscope was
used to examine some of the partially reduced pellets
under different temperatures and loads. A pore size
analyser (Pore sizer 9320, Micromeritics, USA) also
used to characterise the pore size distribution of the
original and reduced pellets.
The sticking tendency of the iron ore pellets under
load was determined by an average drop number test. A
sample weight of about 33–37 g consisting of some eight
pellets was dropped from 50 cm height for 100 times.
After each drop, the weight of the pellets that remain
stuck together was determined. The sticking per cent is
represented by the weight of sticking pellets after each
drop divided by the original weight of the pellets. The
final sticking per cent that corresponds to the last drop
was taken as the degree of sticking.
Table 2 Results of average drop number test of two acidic samples reduced at 950uC under different loads
Results and discussion
X-ray phase analysis and microscopic examination
indicated that hematite (a-Fe2O3) is the predominant
phase in both fluxed pellets. In acidic pellets, iron-
aluminium silicate phases were identified while calcium
and magnesium ferrites were identified in basic pellets.
These phases were formed during firing of pellets at high
temperature (.1200uC) by a solid state reaction between
Fe2O3 and the corresponding constituents of associated
gangue minerals and fluxing materials added in the
pelletising process. The photomicrographs showing the
internal structure of both acidic and basic pellets are
given elsewhere.20 In acidic pellets, silicates of iron and
aluminium were observed whereas in basic pellets,
calcium and magnesium ferrites were formed at the
grain boundaries.
Sticking phenomena
The sticking tendency of the pellets was determined
using average drop number method. Table 2 shows the
results of the average drop number test for two acidic
samples. Sample 1 represents, the pellets reduced at
950uC without load while sample 2 represents, the pellets
reduced at the same temperature under 0?4 kg cm22. It
can be noticed that sample 1 showed some disintegration
as it was subjected to drop test up to 7 times, whereas for
more drops up to 100 times no further weight change
was recorded. The same observation happened in sample
2 but after 55 drops which means that the pellets are
stuck together more strongly compared to sample 1. The
final sticking percentage for the two samples indicates
that they acquired a more or less the same value.
Accordingly, the final sticking value has to be related in
one way or another to the number of drops after which
no weight change occurred. Consequently, a more
reliable parameter was designated and called sticking
index in order to represent sticking phenomenon more
accurately. It is calculated by multiplying final per cent
of sticking and number of drops. The sticking index
values obtained at different temperatures and different
loads give a meticulous measurement for the degree of
sticking. The clustering tendency and per cent of sticking
were found to be dependent on chemical composition,
temperature and applied load.

Load, kg cm22 Total no. of drops No. of drops after which no change occurred Final per cent sticking, %

Sample 1 0 100 7 19
Sample 2 0.4 100 55 21

190 Ironmaking and Steelmaking 2011 VOL 38 NO 3

 Abdel-Halim et al.
a acidic pellets; b basic pellets
1 Photomicrographs of iron ore pellets completely reduced at 1000uC
Chemical composition
Unlike in the basic pellets, the reduced acidic pellets at
temperatures >950uC were stuck together forming
cluster on applying load >0?4 kg cm22 and below which
the sticking of pellets was not considered. The tendency
of iron ore pellets to form clusters during reduction
under load at higher temperatures is affected by the
original chemical composition and physical properties of
pellets. It was found that iron ore sinter having 1?8
basicity behaves fairly well while that of 1?6 basicity
shrunk rapidly.10 This showed a good indication that the
chemical composition of pellets has a pronounced effect
on the physical changes occur during thermal treatment
of pellets. Consequently, acidic iron ore pellets (0?37
basicity) show a greater tendency for clustering than
basic pellets (1?62 basicity). The variation in clustering
tendency is most probably related to the difference in
their chemical and mineralogical composition. The
photomicrographs showing the internal structure of
acidic and basic pellets reduced at 1000uC are given in
2 Effect of reduction temperature on sticking index of
acidic iron ore pellets reduced under different loads
Developed model for reduction mechanism of iron ore pellets
Fig. 1a and b respectively. The basic pellets showed the
formation of a highly porous structure in which a large
number of macropores between iron grains were
developed together with micropores inside grains. The
structure given in Fig. 1a for the acidic pellets shows
that much more dense and relatively large sintered iron
grains are connected forming a coherent matrix with
only large macropores separating dense iron aggregates.
Moreover, fayalite phase was also detected by applying
a suitable etching solution on the polished section of
reduced samples and was also confirmed by X-ray phase
identification. This phase was formed from the solid
state reaction between the wüstite (FexO) resulted from
the reduction of iron oxides and SiO2 associated with
gangue minerals. This phase is barely reduced under the
FexO present reduction conditions. The presence of
silicate phase has a pronounced effect on the enhance-
ment of cluster formation of acidic than in basic reduced
pellets and consequently increasing the sticking
tendency.
Reduction temperature
The influence of temperature on the sticking index
calculated at different loads for acidic iron ore pellets is
represented in Fig. 2. It shows that the temperature has
no measurable influence on the sticking index of samples
reduced under small load ((0?2 kg cm22). At higher
loads, the sticking index increases to large extent with
temperature giving an anomalous value at 850uC and a
minimum value at 900uC. This could be attributed to a
relatively long time taken to reduce pellets at 850uC as
shown in Table 3, since time has a significant effect on
Table 3 Reduction time (min) of acidic pellets reduced
up to 80% at different loads
Load, kg cm22 850uC 950uC 1000uC
0 210 195 165
0.2 255 180 150
0.4 255 210 165
0.57 255 210 195
Ironmaking and Steelmaking 2011 VOL 38 NO 3 191
Abdel-Halim et al. Developed model for reduction mechanism of iron ore pellets
3 Effect of applied load on sticking index of acidic iron
ore pellets reduced at different temperatures
sintering of the reduced iron grains. The minimum
sticking index calculated at 900–950uC was attributed to
a–c-Fe phase transformation and most of sintering
mechanism such as lattice, surface and grain boundary
diffusion is much faster in a-Fe than that in c-Fe.9
Consequently, the sintering of a-Fe produced at 850uC is
relatively higher than in c-Fe that formed at 900–950uC.
The higher index value resulted at 1000uC indicates that
the higher reduction temperature is much more effective
on sintering than reduction time.
Load value
The effect of applied load on the sticking index of acidic
pellets reduced at different temperatures is given in
Fig. 3. It shows no measurable increase in sticking index
value upon applying a load of ,0?4 kg cm22, while
above which the sticking index sharply increased with
increasing load. At higher temperature, the reduced
pellets are stuck together more and the boundaries
between their external surfaces are decreased with
increasing loads. Increasing load allowed for better
stacking of particles inside each pellet, which in turn
increased the points of contact and consequently
enhanced sintering and densification effects. The micro-
structure of the reduced pellets under load (Fig. 4)
showed the formation of clusters at higher temperatures
and loads. This revealed the formation of clusters in
which metallic iron grains were gathered and a large
number of macropores were developed on the expense of
a 0?4 kg cm22; b 0?57 kg cm22
4 Photomicrographs of reduced acidic pellets at 1000uC under different loads
192 Ironmaking and Steelmaking 2011 VOL 38 NO
the internal micropores, giving rise to more contact
points between iron grains and consequently enhanced
sticking tendency.
However, the influence of reduction conditions on the
pore structure developed in the reduced pellets was
investigated by measuring the pore volume, pore
diameter and pore area using high pressure mercury
intrusion pore size analyser. The relationship between
cumulative pore volume and pore diameter for acidic
pellets reduced at 750 and 1000uC under different loads
up to 0?57 kg cm22 is shown in Fig. 5a and b
respectively. In spite of the decrease in total intrusion
volume, the average pore diameter is increased with
temperature. This is an indication that some small pores
collapsed during sintering and others coalesced to
develop large pores. Therefore as temperature increased,
the smallest pores disappeared and large pores emerged.
At higher load a similar structure was observed where
the pellets reduced at 1000uC acquired pores of large
sizes compared to those of pellets reduced at lower
temperature. The slight increase in total pore volume by
load can be attributed to the fissures or cracks formed in
the pellets subjected to load rather than those reduced
without applying load. As the fissures increased, the
total pore volume increased. For samples reduced at
higher temperature and load, more bridging happened
between particles forming clusters which become more
developed with sintering and load.
Kinetic model
The reduction experiments of iron ore pellets under load
revealed that the load plays a pronounced role in the
reduction behaviour of iron ore pellets. To elucidate the
kinetics and mechanism of reduction under load, the
following three procedures were applied:
(i) calculation of activation energy values from
Arrhenius plots
(ii) application of heterogenous gas–solid mathema-
tical formulation
(iii) derivation of reduction mechanism from the
developed reaction model.
Activation energy calculations
The rate controlling mechanism can be determined at
both the initial and the final stages of reduction from the
Arrhenius equation
Kr ~K0 e{Ea =RT (1)
where Kr is the reduction rate constant, K0 is the frequency
factor, R is the gas constant and T is the absolute
3
 Abdel-Halim et al. Developed model for reduction mechanism of iron ore pellets

a 0?0 kg cm22; b 0?57 kg cm22

5 Relationship between cumulative pore volume and pore
diameter for acidic pellets reduced under different tem-
peratures and loads

temperature. The relationships between the logarithm of

the rate of reduction of iron ore pellets (dr/dt) and the
reciprocal of the absolute temperature 1/T are plotted at
both initial (5%) and final (90%) stages of reduction as
given in Fig. 6 for acidic pellets, from which the value of
apparent activation energy Ea can be estimated. The results
obtained from the calculation of Ea for both types of pellet
show that the calculated values at the initial stages of
reduction were in the range of 6?5–13?6 kcal mol21. This
indicates that the process is controlled by a combined effect
of chemical reaction and gaseous diffusion mechanisms.
a initial stages; b final stages
On the other hand, activation energy values of 2?9–
6 Arrhenous plots for reduction of acidic iron ore under
6?4 kcal mol21 were obtained at the final stages of
load
reduction which pointed out that gaseous diffusion
mechanism has the most pronounced effect when pellets
were reduced under load.22 (iii) for the mixed control of chemical reaction and
gaseous diffusion mechanism
Mathematical formulations calculation
t ~Gf (X )zs2 Pfg (X ) (4)
In order to confirm the validity of the above mentioned
* *
mechanisms deduced from the apparent activation where t is the dimentionless time t 5t/tx51,
energy values, the following mathematical formulations where t and tX51 are the time required to reach a
derived by Szekely et al.23–25 were tested against the certain extent of reduction (X) and complete
experimental results: reduction respectively. s2 is the shrinking core
(i) for chemical reaction control mechanism reduction modulus.
Applying line fitting for the mathematical formulations
t ~Gfg (X )~1{(1{X )1=3 (2) representing the different mechanisms indicated that
reduction process at the initial stages of reaction for
both pellets was controlled by the combined mechanism
(ii) for gaseous diffusion control mechanism of chemical reaction and gaseous diffusion. However,
t ~Pfg (X )~1{3(1{X )2=3 z2(1{X ) (3) the same procedure came up with indefinite results at the
final stages of reduction where straight lines were

Table 4 Relation between shrinkage core modulus s2 and Table 5 Experimental parameters of iron ore pellets
mechanism of reduction
Surface area, m2 g21 0.517
2
s Controlling mechanism Porosity, % 32%
Average weight, g 32–35
s2,1 Chemical reaction Gas mixture, % 55%H2, 36%CO, 5%H2O,
1,s2,10 Mixed chemical reaction and gaseous diffusion 3%CO2 and 1%N2
s2.10 Gaseous diffusion Reduction temperature, uC 750–1000

Ironmaking and Steelmaking 2011 VOL 38 NO 3 193

Abdel-Halim et al. Developed model for reduction mechanism of iron ore pellets

obtained for either chemical reaction, gaseous diffusion
or mixed control for both pellets reduced under different
loads. Accordingly, a developed kinetic model was
derived here in after from reaction parameters to
elucidate the reduction mechanism under load as given
in the following section.
Derivation of reduction mechanism from reaction model
parameters
In order to have good comprehension about the effect of
both reduction temperature and applying loads besides
finding out which mechanism controls the reduction
process, a mathematical modelling for kinetics and
mechanism was used. According to the grain model
developed by Szekely et al.,23–25 the different controlling
mechanisms were represented by equations (2)–(4). The
dimensionless time (t*) can be defined according to the
following equation
   Table 4. To calculate the value of s2, some experimental
bk Ag CCS
t ~ CAS { t (5)
rs Fg Vg KE
where, b is the mole fraction, k is Boltzmann constant,
Ag is the grain area, Fg is the grain shape factor, rs is the
solid density, Vg is the grain volume, CAS is the
concentration of gaseous reactant ‘A’ on surface, CCS
is the concentration of gaseous product ‘C’ on surface,
KE is the equilibrium constant, and t is time.
The shrinking core reaction modulus is defined by the
following formula
" #1=2
1
2 Vp kFp Ag (1{e)(1{ KE )
s ~ (6)
Ap 2De Fg Vg
where Vp is the particle volume, Ap is the particle area,
Fp is the particle shape factor, e is the porosity, and De is
the effective diffusivity.
According to equation (4), the shrinking core reaction
modulus (s2) can be used as the factor which determines
the relative contribution of both gaseous diffusion
mechanism and chemical reaction in the mixed control
formula. Hence, the mechanism of reduction can be
estimated according to the value of s2 as shown in
parameters (given in Table 5) should be incorporated.
The values of s2 were calculated for different extents of
reduction (5, 25, 70 and 90%) in the temperature range
of 750–1000uC and under different loads (Fig. 7). It was
found that s2 has different values between 1 and 10;
consequently the reduction process is controlled by

a acidic pellets; b basic pellets a acidic pellets; b basic pellets

7 Effect of reduction temperature on value of shrinking 8 Effect of reduction temperature on value of shrinking
core reaction modulus at different extents of reduction core reaction modulus for iron ore pellets reduced
and under load 0?4 kg cm22 under different loads

194 Ironmaking and Steelmaking 2011 VOL 38 NO 3

 Abdel-Halim et al.
mixed mechanisms. This is in agreement with the
controlling mechanism derived from the values of the
activation energy.26 As temperature increased, the value
of the shrinking core modulus increased. At the early
stages of reduction, the values of s2 were highest
especially at lower loads whereas at intermediate and
final stages of reduction, the temperature has a less
pronounced effect on the value of s2. The relation
between s2 and temperature at different loads for both
iron ore pellets at 5% extent of reduction is given in
Fig. 8. It can generally be seen that the value of s2
depends on both the reduction temperature and applied
load. The values of s2 increase steadily by either
increasing the temperature or decreasing the load. This
means that the contribution of gaseous diffusion is more
pronounced by increasing the temperature and
decreased with increasing applied load. The increase in
the value of s2 by increasing temperature can be
attributed to the enhancement of the chemical reaction
caused by increasing temperature. Accordingly, the
diffusion of the gas is the slowest step and the
contribution of gaseous diffusion in the controlling
mechanism decreases with temperature. The variation of
s2 with load can be attributed to the change in the
structure of pellets during reduction. Figure 9 shows the
a acidic pellets; b basic pellets
9 Effect of load and extent of reduction on porosity of
partially reduced iron ore pellets at 800 and 1000uC
Developed model for reduction mechanism of iron ore pellets
relationship between total porosity and loads at
different extents of reduction for both acidic and basic
pellets. It was observed that at the early intermediate
stages (40% extent) of reduction, the per cent of porosity
increased by increasing the load and temperature. Also,
the pellets become more porous with the progress of
reduction process but near the final stages of reduction
(85% reduction extent) the effect of load on the per cent
of porosity was less significant.
In order to investigate the effect of load and
temperature on the mechanism of reduction, particularly
in the mixed control mechanism region, the ratio of the
contribution of chemical reaction mechanism to gas
diffusion mechanism, called hereinafter the mixed
control ratio Q, was calculated according to the
following formula
Gfg (X )
Q~ (7)
s2 Pfg (X )
This ratio determines to some extent the contribution of
each of the mechanisms in the mixed control. Figure 10
shows the relation between Q and reduction extent (X) at
different temperatures for both pellets. It is observed
that at the early stages of reduction this ratio shows a
a acidic pellets; b basic pellets
10 Mixed control ration of iron ore pellets reduced under
different loads at 750uC
Ironmaking and Steelmaking 2011 VOL 38 NO 3 195
Abdel-Halim et al. Developed model for reduction mechanism of iron ore pellets
higher value which in turn indicates that the contribu-
tion of a chemical reaction mechanism is more effective
than that of a gaseous diffusion mechanism. As the
reduction increases to 15–20% a sharp drop in the value
of Q is shown and kept more or less constant for most of
the reduction course at about 1–2. This is an indication
that the contribution of gaseous diffusion control
increases on the expense of the chemical reaction control
share in the mixed control reaction. At the final stages of
reduction, the values of Q lie around 1, which means the
contributions of both chemical mechanism and gas
diffusion mechanism are equal. On the other hand, the
effect of load can be pronounced as observed at the early
stages of reduction where the values of Q are higher upon
applying higher loads which in turn direct effective
contribution of reaction control mechanism towards the
chemical reaction. As the per cent of reduction increases
the effect of load decreased gradually and nearly
disappeared at the final stages of reduction.
Conclusion
The present work studied the gaseous reduction of
commercial iron ore pellets at 750–1000uC under
different loads ranged from 0?2 to 0?57 kg cm22. The
sticking phenomenon accompanying reduction of iron
ore pellets under load was investigated. The sticking
tendency was found to be dependent on temperature,
chemical composition and applied load. Increasing the
load allowed for close packing of the particles which, in
turn, increased the points of contact between metallic
iron and consequently enhanced sintering and densifica-
tion processes. The sticking phenomena are observed
only for acidic pellets where the presence of silicate
phase has pronounced effect on the enhancement of
clustering tendency.
The experimental results were used for determining
the reduction mechanism using the conventional meth-
ods of calculating the apparent activation energy values
as well as applying the mathematical formulations
corresponding to the different gas–solid reaction
mechanisms. In the present work, a developed kinetic
model was demonstrated depending on the calculation
of the shrinking core reaction modulus and the mixed
control ratio. The model deals with the causes which do
not come up with definite results when handled by the
196 Ironmaking and Steelmaking 2011 VOL 38 NO
above mentioned conventional methods. The model
enables good analysis about the actual effect of
reduction temperature and applied load upon the
controlling mechanism. It also indicates the relative
effects of the different mechanisms for case which are
controlled by mixed mechanisms.
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3
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